2,4-滴胺

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of N-(3-cyano-phenyl)-2-(2,4-dichloro-phenoxyacetamide (70.0 mg, 0.22 mmol), sodium azide (42.9 mg, 0.66 mmol) and triethylamine hydrochloride (45.4 mg, 0.33 mmol) in N-methylpyrrolidone (6 ml) (NMP) was stirred at 150° C. under nitrogen overnight. After cooling, the reaction mixture was diluted with water, acidified to PH 1 with 10% v/v hydrochloric acid, and extracted with ethyl acetate. The organic phase was washed with brine, dried (MgSO4 anh), and concentrated. The residue was purified by silica gel flash column chromatography (CH2CH2:MeOH=3:1) to give 2-(2,4-dichloro-phenoxy)-N-[3-(1H-tetrazole-5-yl)-phenyl]-acetamide as a solid (57.2 mg, 71.6% yield). After cooling extracted with ethyl acetate The organic phase was washed with brine dried (MgSO4 anh) concentrated The residue was purified by silica gel flash column chromatography (CH2CH2:MeOH=3:1)